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ASTA

CLEANLINESS SPECIFICATIONS
FOR
SPICES, SEEDS, AND HERBS

(FOREIGN and DOMESTICALLY PRODUCED)

REVISED 2007

American Spice Trade Association


www.astaspice.org

2025 M St, NW Suite 800


Washington, DC 20036
E-Mail: info@astapice.org
Phone: (202) 367-1127
Fax: (202) 367-2127
PREFACE
ASTA adopted the original Cleanliness Specifications for spices, seeds and herbs in 1969 and they have been
revised numerous times. The goal of the specifications has remained unchanged over the years. ASTA seeks to
ensure that the spices, seeds and herbs traded by its members meet FDA’s Food Safety and Security guidance
before being further processed into acceptable finished products for consumption at the consumer, food service
and industrial level.
The ASTA Cleanliness Specifications were designed to meet or exceed the United States Food and Drug
Administration (FDA) Defect Action Levels (DAL). ASTA’s Cleanliness Specifications establish limits for
macroscopic extraneous matter for domestic and imported spices, seeds and herbs coming into the United States.
The Cleanliness Specifications also include microscopic filth limits (e.g. insect fragments, rodent hairs) for
specific products that are also addressed by the FDA DALs.
The Cleanliness Specifications do not address microbiological contamination of spices or the adulteration of
spices through the inclusion of food dyes or other materials not permitted in spices. In the United States such
instances are governed by the Federal Food, Drug, and Cosmetic Act and the relevant regulations and policies of
the Food and Drug Administration.

The ASTA Cleanliness Specifications are widely recognized within the spice industry and members are
encouraged to apply them in transactions between buyers and sellers of spices, including instances when an
ASTA contract is utilized.

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CLEANLINESS SPECIFICATIONS

For purposes of these Specifications, extraneous matter is defined as everything foreign to the product itself and
includes, but is not restricted to: stones, dirt, wire, string, stems, sticks, nontoxic foreign seeds, excreta, manure
and animal contamination.
The level of contaminants permitted under these Specifications must fall below those shown on the following
table, except for the column ∆ "Whole Insects, Dead" which cannot exceed the limits shown.

CLEANLINESS ∆ WHOLE INSECT EXTRANEOUS/


SPECIFICATIONS INSECTS, EXCRETA, EXCRETA, DEFILED/ FOREIGN
DEAD MAMMALIAN OTHER MOLD INFESTED MATTER
Name of By By By % By % By % By
Spice, Seed or Herb Count Mg./Lb. Mg./Lb. Wgt. Wgt. Wgt.
Allspice 2 5 5.0 2.00 1.00 0.50
Anise 4 3 5.0 1.00 1.00 1.00
Sweet Basil 2 1 2.0 1.00 1.00 0.50 ■
Caraway 4 3 10.0 1.00 1.00 0.50
Cardamom 4 3 1.0 1.00 1.00 0.50
Cassia 2 1 1.0 5.00 2.50 0.50
Cinnamon 2 1 2.0 1.00 1.00 0.50
Celery Seed 4 3 3.0 1.00 1.00 0.50
Chillies 4 1 8.0 3.00 2.50 0.50
Cloves* 4 5 8.0 1.00 1.00 1.00 *
Coriander 4 3 10.0 1.00 1.00 0.50
Cumin Seed 4 3 5.0 1.00 1.00 0.50
Dill Seed 4 3 2.0 1.00 1.00 0.50
Fennel Seed SF(2) SF(2) SF(2) 1.00 1.00 0.50
Ginger 4 3 3.0 SF(3) SF(3) 1.00
Laurel Leaves** 2 1 10.0 2.00 2.50 0.50
Mace 4 3 1.0 2.00 1.00 0.50
Marjoram 3 1 10.0 1.00 1.00 1.00 ■
Nutmeg (Broken) 4 5 1.0 SF(4) SF(4) 0.50
Nutmeg (Whole) 4 0 0.0 SF(5) SF(5) 0.00
Oregano*** 3 1 10.0 1.00 1.00 1.00 ■
Black Pepper 2 1 5.0 SF(6) SF(6) 1.00
White Pepper**** 2 1 1.0 SF(7) SF(7) 0.50
Poppy Seed 2 3 3.0 1.00 1.00 0.50
Rosemary Leaves 2 1 4.0 1.00 1.00 0.50 ■
Sage** 2 1 4.0 1.00 1.00 0.50
Savory 2 1 10.0 1.00 1.00 0.50 ■
Sesame Seed 4 5 10.0 1.00 1.00 0.50
Sesame Seed, Hulled 4 5 1.0 1.00 1.00 0.50
Tarragon 2 1 1.0 1.00 1.00 0.50 ■
Thyme 4 1 5.0 1.00 1.00 0.50 ■
Turmeric 3 5 5.0 3.00 2.50 0.50

Cleanliness Specifications - Footnotes:

* Clove Stems: Less than (<) 5% allowance by weight for unattached clove stems over and above the tolerance
for Other Extraneous Matter is permitted.

** Laurel Leaves: "Stems" will be reported separately for economic purposes and will not represent a

Sage: pass/fail criteria.

*** Oregano: Sumac negative-Analysis for presence of Sumac shall not be mandatory if samples are marked
"Product of Mexico."

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**** White Pepper: "Percent Black Pepper" will be reported separately for economic purposes and will not represent
a pass/fail criteria.

(2) Fennel Seed: In the case of Fennel Seed, if 20% or more of the subsamples contain any rodent, other excreta or
whole insects, or an average of 3 mg/lb or more of mammalian excreta, the lot must be
reconditioned.

(3) Ginger: More than 3% moldy pieces and/or insect infested pieces by weight.

(4) Broken Nutmeg: More than 5% mold/insect defiled combined by weight.

(5) Whole Nutmeg: More than 10% insect infested and/or moldy pieces, with a maximum of 5% insect defiled pieces
by count.

(6) Black Pepper: 1% moldy and/or infested pieces by weight.

(7) White Pepper: 1% moldy and/or infested pieces by weight.

∆ Whole Insects, Dead: Cannot exceed the limits shown.

■ Extraneous Matter: Includes other plant material, e. g. foreign leaves

GROUND PROCESSED SPICE *

(Cannot exceed limit shown)

Whole Insect Other Rats/ Animal


Spices Equivalent Fragments Mites Insects Mouse Hairs
Insects Hairs

Ground Average of Average of


Paprika more than 75 more than
fragments 11 rodent
/25g hairs/25g

* Microanalytical Methods for Paprika and Ground Capsicums can be found in the “Analytical Procedures” section
of this book.

FDA’s Defect Action Levels can be found at:


http://www.fda.gov/food/guidancecomplianceregulatoryinformation/guidancedocuments/sanitation/ucm056174.htm#CHPT3

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IN ADDITION TO THE PRECEDING SPECIFICATIONS, A LOT MUST ALSO BE
RECONDITIONED:

A. MAMMALIAN EXCRETA -
if the average of the total number of subsamples exceeds the listed milligram per pound Specification.
Exception: In the case of fennel seed, see footnote (2).

B. OTHER EXCRETA -

if the average weight expressed as milligrams per pound for all subdivisions of the sample exceeds the
specified values shown in the table.
Exception: In the case of fennel, see footnote (2).

NOTE: The Food and Drug Administration specifies only mammalian excreta, ASTA will count all types of
non-mammalian excreta as Other Excreta. FDA does retain the right to detain merchandise containing excessive
amounts of excreta which is of non-mammalian origin on the basis that the merchandise was exposed to
Insanitary Conditions.

C. INSECTS -

if the total number of whole dead insects found in the total number of the subsamples exceeds the specified
value shown in the table.

if live insects are found in the original sample reconditioning is to include fumigating. If the number of live
and dead insects exceed the cleanliness specification for whole dead insects for that spice, then
reconditioning must also include sifting and blowing, requiring samples to be drawn and analyzed.
Exceptions:

a. In the case of fennel seed, if 20% or more of the subsamples contain any whole insects, the lot
must be reconditioned. (For example, if two or more subsamples of a ten-unit sample each
contains one whole insect, the lot must be reconditioned.)

b. If the number of live insects found in the total number of subsamples are less than the
cleanliness specifications for whole insects for that spice, the lot must be fumigated and then
resampled.

c. If it appears to the unaided eye that 50 or more mites and psocids are present, the lot must be
fumigated, sifted and blown. Mites and/or psocids are not to be counted as insects.

D. MOLD -

if mold is present, as expressed by percent by weight of the total quantity of spice in all subsamples, in
excess of the specified values shown in the table. A product is classified as moldy if it contains mold,
visible to the naked eye, exceeding 1/4 of its surface area and confirmed by the presence of mycelial
filaments and spores when examined with the aid of a microscope (40 X magnification or less).

E. INSECT DEFILED/INFESTED -

if the total sample quantity exceeds the specified values shown in the table expressed as percent by weight
of insect infested, bored, or otherwise defiled seeds, leaves or roots. Before reconditioning a lot is
considered defiled whenever a sample shows visible evidence of webbing or definite insect feeding.

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F. RECONDITIONING AND RECONDITIONED ITEMS -

Reconditioning may include, but shall not be limited to, techniques such as fumigating, washing, cutting,
sifting, aspirating and blowing.

Insect channels or insect-bored holes in reconditioned spices will not be counted as insect defiled, as they
would in the examination of non-reconditioned spices, provided there are no insects, webbing or excreta in
those channels or holes.

G. LIGHT BERRIES - Black Pepper -

if the light berries, though not considered extraneous matter, exceed 4% by weight.

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SAMPLING AND ANALYTICAL PROCEDURES

A. SAMPLING -

i. Each lot distinguished by specific chop marks and/or numbers must be sampled/analyzed
separately. A lot shall be defined as not to exceed one container load, where applicable. No
commingling is permitted.

ii. In sampling merchandise for analysis under these specifications, the number of samples drawn
must be equal to the square root of the packages, bags or containers in the lot with a maximum
of ten samples drawn. In the event that this is for ground/crushed processed spices the number
of samples drawn must be six.

iii. The sample size shall be 3/4 to 1 pound for the high density items. These include: Black and
White Pepper, Cassia, Cinnamon (Seychelle), Nutmeg (Whole and Broken), Ginger, Cloves,
Allspice/Pimento, Turmeric, Celery Seed, Poppy Seed, Sesame Seed, Caraway Seed,
Cardamom Seed, Anise Seed, Coriander Seed, Cumin Seed, Dill Seed, and Fennel Seed.

The sample size shall be 1/2 to 3/4 of a pound for the low density items. These include:
Chillies, Capsicums, Mace, Sage, Oregano Leaves, Basil Leaves, Laurel Leaves, Thyme
Leaves, Rosemary Leaves, Tarragon Leaves, Marjoram Leaves and Savory Leaves.

iv. The sampling size shall be 4-6 ounces (113-170 grams) for ground/crushed processed spices.

v. In all cases, each subsample must be analyzed. In the case of high and low density items the
entire sample must be analyzed, in the samples of ground and crushed processed spices the
amount to be analyzed is determined by the method used.

B. PROCEDURES -

Utilize the appropriate methods as given under the “Analytical Procedures” section of this manual.

C. RESAMPLING/REANALYSIS -

i. No resampling or reanalysis is permitted except in those instances where fumigation and/or


reconditioning has taken place.

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ANALYTICAL PROCEDURES

7
ASTA ANALYTICAL METHODS

Method 14.0
Light Berries and Extraneous Matter in Black and White Pepper

Purpose: To determine the amount of light berries and extraneous matter in black or white pepper.

A. Apparatus:

1. A standard pepper sieve, (No. 9 1/2 round screen with a frame 18 to 22 inches in diameter and 2 3/4
inches in height. The bottom is a metal sheet perforated with round holes of 7/64 inch in diameter,
with an average of 5 1/2 holes per linear inch. Screen only with standard pepper sieve obtainable
from: McNichols Company, 5501 Gray Street, Tampa, Florida 33609 (813) 876-4100 or (800) 237-
3820. U.S. Standard No. 8 sieve (0.0937 in. or 2.38 square mm opening) provide equivalent sieve
opening.

2. Balance -- sensitivity 0.01 g.

3. Beaker, 600 ml. Griffin, Low form, pyrex approximately 85 mm. in diameter and 120 mm. in height
is recommended. (Note 1).

4. Blotting paper or other similar absorbent material.

5. Tweezers.

6. Stereoscopic, Binocular, wide-field microscope (40-50x).

B. Reagents:

1. Alcohol-water solution of a specific gravity 0.80-0.82 at 25°/25°. The alcohol may be ethanol,
denatured ethanol (Note 2) or isopropanol.

C. Preparation of Sample:

1. The number of samples drawn must be equal to the square root of the packages, bags, or containers
in the lot, with maximum of 10 samples drawn.

2. The sample size shall be 3/4 to l pound (340 g to 454 g).

3. Each entire subsample must be analyzed.

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ASTA ANALYTICAL METHODS

Method 14.0
Light Berries and Extraneous Matter in Black and White Pepper

D. Procedure:

1. To Determine Excreta, Insects, Mites, Psocids, Mold, and Percent Black Pepper in White
Pepper:
a. Weigh each sub-sample to the nearest gram. Sprinkle and examine a small portion at a time,
with a good light and against a white background into a standard pepper sieve. Pick out any
bird, rodent, or other animal excreta. Separate mammalian from non-mammalian excreta.
Weigh to the nearest 0.1 mg and record. Do not remove other extraneous/foreign material at
this time.
b. Shake pepper sieve moderately back and forth, examine siftings collected on white
background for live and dead insects and for excreta.
c. Accumulate the siftings.
d. Mix sub-sample of pepper on sieve and weight 50 g of aliquot into a pan. Hand-pick moldy
peppercorns and weigh. In case of white pepper, additionally hand pick for black
peppercorns (with skin coat attached) and record. Each sub-sample is examined in sequence
in a similar manner and the results are averaged.

2. Extraneous/Foreign Matter by Sifting:


a. Weigh to nearest 0.1 g the cumulated siftings and calculate the percentage by weight.
Percent siftings must be determined after the removal of small berries that pass through the
pepper sieve. (See Calculations)

3. Light Berry Determination for Black Pepper:


a. Combine sufficient material from each sub-sample to give a composite sample of
approximately 5 lbs. Mix composite well.
b. Form the composite into a pile shaped like a cone. Quarter the cone designating each
quarter as A, B, C, or D in a clockwise sequence.
c. Set aside two opposite quarters such as A and C.
d. Mix and reduce each quarter separately.
e. Remove a 50.0 g sample from each reduced quarter.
f. Place the weighed sample in the 600 mL Griffin, low-form pyrex beaker and add 300 mL of
the alcohol-water solution.
g. Stir the material in the beaker with a spoon and allow to settle two minutes; then spoon off
the berries which float.
h. Repeat the stirring, settling and removal of the floating berries until two successive
additional stirrings raise no more berries to the surface. Remove only the berries that
actually float (Note 3).
i. Blot the removed berries to free them from excess liquid and spread them out to dry on a
piece of paper towel or other absorbent material.

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ASTA ANALYTICAL METHODS

Method 14.0
Light Berries and Extraneous Matter in Pepper

j. Air dry for one hour and weigh the air dried light berries to the nearest 0.01 g and calculate
and report the percent of light berries to the nearest 0.1%.
(See Calculations)
k. If the range of two determinations is not over 0.8%, the two determinations shall be averaged
and reported as percent light berries. If the difference is greater than 0.8%, determine the
light berries in a third sample obtained from either quarter B or D. Average all three values
and report as percent light berries.
4. Extraneous/Foreign Matter by Hand Picking
a. From the two opposite quarters set aside for light berries determination such as A & C,
weigh 100 grams from each and hand pick for any sticks, stones, stems, foreign seeds, other
extraneous matter and make note of its nature.
b. Weigh the pickings and calculate. (See Calculations)
E. Calculations:
Wt. of combined sifting (g)
% Extraneous/Foreign Matter by Sifting = ____________________________________________________ x 100
Combined wt. of sub-samples (g)

weight of light berries (g)


% Light Berries = ____________________________________________________________ x 100
weight of samples (50 g)

A (in grams) + C (in grams)


__________________________________________________
% Extraneous/Foreign Matter by Hand Picking =
2
F. Statistics:
TBD
G. Notes:

1. Other transparent beakers may be used, but they should be between 75 and 100 mm. in diameter and
between 100 and 140 mm in height.

2. Specially denatured alcohols no. 3A, 23A, or 30 are recommended.


a. SDA no. 3A: 5 gallons of methyl alcohol plus 100 gallons 95% ethyl alcohol.
b. SDA no. 23A: 10 gallons USP acetone plus 100 gallons 95% ethyl alcohol.
c. SDA no. 30: 10 gallons methyl alcohol plus 100 gallons 95% ethyl alcohol.

3. Some berries may remain suspended some distance below the surface of the liquid. These are not
considered as floaters.
H. References:
Macroanalytical Procedures Manual 1984, Chapter 5.
Revised January, 1997

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ASTA ANALYTICAL METHODS

Method 14.1
Extraneous Matter in Spices (Excluding Black and White Pepper)

Purpose: To determine the amount of extraneous matter in spices (excluding black and white
pepper).

A. Apparatus:

1. A standard pepper sieve, (No. 9 1/2 round screen with a frame 18 to 22 inches in diameter and 2 3/4
inches in height. The bottom is a metal sheet perforated with round holes of 7/64 inch in diameter,
with an average of 5 1/2 holes per linear inch. Screen only with standard pepper sieve obtainable
from: McNichols Company, 5501 Gray Street, Tampa, Florida 33609 (813) 876-4100 or (800) 237-
3820. U.S. Standard No. 8 sieve (0.0937 in. or 2.38 square mm opening) provide equivalent sieve
opening.

2. Balance -- sensitivity 0.01 g.

3. Tweezers

4. Binocular, wide-field microscope (40-50x).

B. Reagents:

None required.

C. Preparation of Sample:

1. The number of samples drawn must be equal to the square root of the package, bags or containers in
the lot with a maximum of ten samples drawn.

2. The sample size shall be 3/4 to 1 pound for high density items. These include: Cassia, Cinnamon
(Seychelle), Nutmeg (Whole and Broken), Ginger, Cloves, Allspice/Pimento, Turmeric, Celery
Seed, Poppy Seed, Sesame Seed, Caraway Seed, Cardamom Seed, Anise Seed, Coriander Seed,
Cumin Seed, Dill Seed, and Fennel Seed.

3. The sample size shall be 1/2 to 3/4 of a pound for low density items. These include: Chillies,
Capsicums, Mace, Sage, Oregano Leaves, Basil Leaves, Laurel Leaves, Thyme Leaves, Rosemary
Leaves, Tarragon Leaves, Marjoram Leaves and Savory Leaves.

4. Regardless of sample size, the entire subsample must be analyzed.

11
ASTA ANALYTICAL METHODS

Method 14.1
Extraneous Matter in Spices (Excluding Pepper)

D. Procedure:

1. Whole and Broken Nutmegs:

Whole Nutmegs:
a. Weigh and shake each subsample on the sieve. Examine siftings for live and dead insects,
extraneous matter and mammalian or other excreta.
b. Select at random 100 Nutmegs from each subsample. Cut the Nutmegs in half longitudinally.
Examine the cut surfaces of each Nutmeg for evidence of insects or insect damage and
presence of mold filaments. Report as rejects Nutmegs containing insects or insect parts,
insect excreta, insect channeling, and those showing mold filaments on 25% or more of the
cut surface of each. (Note 3) Check borderline or doubtful specimens using magnification.
Report results for Insect Defiled/Infested and for Mold separately for each subsample in % by
count and average.

Broken Nutmegs:
a. Weigh and shake each subsample on the sieve. Examine siftings for live and dead insects,
extraneous matter. (Note 1)
b. Mix thoroughly, weigh out 50 grams of each subsample and examine the surfaces of the
Nutmegs for evidence of insects or insect damage and presence of mold filaments. Report as
rejects Nutmegs containing insects or insect parts, excreta, insect channeling, and those
showing mold filaments on 25% or more of the cut surface of each. (Note 3) Check borderline
or doubtful specimens using magnification. Report results of each subsample in % by weight
and average. Results of Insect Defiled/Infested and Mold can be combined in the case of
Broken Nutmegs. (Note 1)

2. Chillies:

a. The individual subsample is weighed, shaken from the bag, a small portion at a time, with a
good light, on the sieve with white paper beneath. As the chillies are discharged on the sieve,
they are examined for extraneous/foreign matter, mammalian, or other excreta. (Note 1)

b. When the entire sample is on the sieve, it is shaken back and forth a few times. The siftings
on the white paper are also examined for live and dead insects, mammalian, or other excreta.

12
ASTA ANALYTICAL METHODS

Method 14.1
Extraneous Matter in Spices (Excluding Pepper)

c. The sample is mixed and a 25 gram portion for chillies up to 2 1/2 inches in length or 100
gram portion for chillies over 2 1/2 inches in length is taken at random for examination of
mold or insect defiled/infested chillies. (Note 3) The chillies are broken and examined inside.
Moldy chillies (mold exceeding 1/4 of its area) or insect defiled/infested pods are weighed
and % by weight determined.
d. Each sample representing the lot is done in sequence in this manner.

3. Basil, Marjoram, Oregano (Note 2), Rosemary Leaves, Savory, Tarragon, and Thyme:
a. The individual subsamples are weighed. Each subsample is shaken from the bag, a small
portion at a time on white paper, with good light.
b. As the sample is discharged and spread out on the paper, examine and pick out live and dead
insects, mammalian and other excreta, mold and insect defiled/infested pieces. (Note 1 and
Note 3)
c. Report by count (Whole Insects) or by weight (Mammalian Excreta. Other Excreta, Mold and
Insect Defiled/Infested Pieces) on the Certificates of Analysis.
d. Extraneous/Foreign Matter is defined as everything foreign to the product itself and includes,
but is not restricted to: stones, dirt, wire, string, stems, sticks, nontoxic foreign seeds and hair
and other plant materials, e.g. foreign leaves. (Note 5)
e. From a composite of the subsamples weigh out and hand pick 100 grams of sample for
extraneous/foreign matter.
f. Record results in percent by weight.

4. Anise Seed, Caraway Seed, Celery Seed, Cloves, Coriander, Cumin Seed, Dill Seed, Fennel Seed,
Mace (siftings), Poppy Seed, Sesame Seed, Hulled Sesame Seed:

a. The individual subsamples are weighed. Each subsample is shaken from the bag, a small
portion at a time on white paper, with good light.
b. As the sample is discharged and spread out on the paper, examine and pick out live and dead
insects, mammalian or other excreta, mold and insect defiled/infested pieces. (Note 1, Note 3)
c. Report by count (Whole Insects) or by weight (Mammalian Excreta. Other Excreta, Mold and
Insect Defiled/Infested Pieces).
d. Extraneous/Foreign Matter is defined as everything foreign to the product itself and includes,
but is not restricted to: stones, dirt, wire, string, stems, sticks, nontoxic foreign seeds and hair.

13
ASTA ANALYTICAL METHODS

Method 14.1
Extraneous Matter in Spices (Excluding Pepper)

e. From a composite of the subsamples weigh out and hand pick 50 grams of sample for
extraneous/foreign matter.
f. Record results in percent by weight.

5. Allspice/Pimento, Whole Cardamom, Broken Cassia, Madagascar and Seychelle Cinnamon,


Ginger, Laurel Leaves (Fig. 1), Mace (whole), Sage, Turmeric (Note 4, Note 5):
a. The individual subsample is weighed, shaken from the bag, a small portion at a time, with
a good light, on the sieve with white paper beneath. As the sample is discharged on the
sieve, examine for extraneous/foreign matter, mammalian, or other excreta.
b. When the entire sample is on the sieve, it is shaken back and forth a few times. The
siftings on the white paper are also examined for live and dead insects, mammalian, or
other excreta. (Note 1)
c. Examine entire sample for mold or insect defiled/infested pieces. (Note 3)
d. Report by count (Whole Insects) or by weight in milligrams (Mammalian Excreta, Other
Excreta).
e. Each sample representing the lot is done in sequence in this manner.

6. Cassia Sticks or Vera AA Cassia:


a. Break each stick separately from the entire subsample into pieces with a hammer or
weight.
b. Examine the pieces for mold or insect defiled/infested pieces. (Note 3)
c. The entire stick is considered in the calculations where evidence of contamination is
found.
d. Report results of each subsample in % by weight in milligrams.

E. Calculations:

1. Excreta mg/lb = Weight Excreta (mg) 454g


x
Weight of Product (g) 1 lb.

2. % Moldy/Insect Defiled/Infested Product = Weight Reject Product (g) x 100


Weight Product (g)

3. % Siftings = Weight Siftings (g) x 100


Weight Product (g)

4. %Extraneous Matter = Weight Extraneous Matter (g) x 100


Weight Product (g)

14
ASTA ANALYTICAL METHODS

Method 14.1
Extraneous Matter in Spices (Excluding Pepper)

F. Statistics:

TBD

G. Notes:

1. Calculate the average milligrams of mammalian excreta and the average milligram of other excreta
across all of the subsamples analyzed and report each value separately, and as mg/lb (see
Calculations).

2. In the case of Oregano, analysis for the presence of Sumac must be performed (See Method 26.0).
However, if the samples are marked "Product of Mexico", analysis for the presence of Sumac shall
not be mandatory.

3 . Classification of Mold and Insect Defiled - Insect Defiled -- Any product material exhibiting definite
evidence of insect feeding or webbing.

Mold -- any material bearing mold, visible to the naked eye, exceeding 1/4 of its area and confirmed
by the presence of mycelial filaments and spores when examined the aid of a microscope (40X
magnification or less).

4. In the case of Sage and Bay leaves only, a separate column will be used on the Certificate of
Analysis to report "Stems." This information will be for economic purposes only and will not
represent a pass/fail criteria.

15
ASTA ANALYTICAL METHODS

Method 14.1
Extraneous Matter in Spices (Excluding Pepper)

5. The definitions of extraneous plant material/stem:

SAGE - If any pithy plant material exceeds one (1) millimeter in diameter at any point on its
contiguous body, the attached leaves are stripped and if the length exceeds twelve and a half
(12.5) millimeters, the remaining material is defined as a stem. In addition, if any pithy plant
material exceeds two (2) millimeters in diameter at any point, it is considered to be a stem
regardless of its length. That material is to be weighed and the total weight of stems reported as
a percentage.

BAY (LAUREL) LEAVES - If any pithy plant material, excluding the "bud," exceeds one (1)
millimeter in diameter at any point on its contiguous body, the attached leaves are stripped and if
the length exceeds twelve and a half (12.5) millimeters, the remaining material is defined as a
stem. In addition, if any pithy plant material exceeds two (2) millimeters in diameter at any
point, it is considered to be a stem regardless of its length. That material is to be weighed and
the total weight of stems reported as a percentage.

ROSEMARY and SAVORY - The analyst establishes an average size of the leaves in a
particular lot. Any pithy plant material other than the leaves exceeding that size/dimension is
defined as extraneous matter.

THYME - If any pithy plant material exceeds the suggested length of twelve and a half (12.5)
millimeters (1/2"), it is defined as extraneous matter.

CLOVES - If a stem attached to a clove is greater in length than the clove itself, it shall be
broken off and counted as a clove stem.

OREGANO - If any pithy plant material exceeds one (1) millimeter in diameter at any point on
its contiguous body, the attached leaves are stripped and if the length exceeds twelve and a half
(12.5) millimeters (1/2"), the-remaining material is defined as extraneous matter. In addition, if
any pithy plant material exceeds two (2) millimeters in diameter at any point, it is considered to
be extraneous matter regardless of its length.

SWEET BASIL - If any pithy plant material exceeds one (1) millimeter in diameter at any point
on its contiguous body, the attached leaves are stripped and if the length exceeds twelve and a
half (12.5) millimeters (1/2"), the remaining material is defined as extraneous matter. In
addition, if any pithy plant material exceeds two (2) millimeters in diameter at any point, it is
considered to be extraneous matter regardless of its length.

H. References:

Macronalytical Procedures Manual (MPM) 1984, Chapter V.

Revised January, 1997

16
ASTA ANALYTICAL METHODS

Method 22.1
Microanalytical Analysis of Paprika

Purpose: To isolate extraneous material of insect, rodent, other animal and bird origin
from ground paprika for microscopic detection and enumeration.

A. Apparatus:

1. Stereoscopic binocular microscope - wide field with following minimum specifications: 3


parfocal objectives - 1X, 3 X and 6X or 7.5X; paired 10X wide field oculars, mounted on a base
and capable of illumination by reflected light. Ordinarily 30X magnification is used for routine
examination of filter papers. Confirmation of suspect material at higher magnification may be
required.

2. Microscope illuminator - preferably with a transformer or rheostat to vary light intensity, a


focusing adjustment to give uniformly lighted field of view, and blue-white color from a cool
low-voltage source.

3. Wildman trap flask - consists of a 2L Erlenmeyer flask into which is inserted a close-fitting
rubber stopper supported on a stiff metal rod, 3/16" diam., and about 4" longer than height of
flask. Rod is threaded at lower end and furnished with nuts and washers to hold it in place on the
stopper. Countersink lower nut and washer in the rubber stopper to prevent striking flask.

4. Filter paper: a) 32 cm folded rapid flow (S & S 588, or equivalent).


b) 9 cm high wet strength, ruled, 5mm apart (S&S #8 or equivalent).

5. Hirsch funnel, porcelain, 56 mm plate diameter.

6. Büchner funnel, porcelain, 114 mm diameter.

7. Suction flask to provide suction by means of an H2O aspirator or electric vacuum pump.

8. Sieve U.S. Standard No. 230, 8" or 12" diameter (plain-not twill weave).

9. Magnetic stirrer - hot plate.

10. Teflon coated magnetic stirring bar, 1 3/4" - 2" x 3/8" (44.4 mm - 50.8 mm x 9.5 mm).

11. Beakers, glass - 1 liter, funnels, glass or metal, 6" diameter or greater

17
ASTA ANALYTICAL METHODS

Method 22.1
Microanalytical Analysis of Paprika

B. Reagents

1. Isopropanol and 40% isopropanol in water.

2. Premix Tween 80-40% isopropanol-Tetrasodium EDTA: mix 250mL of (a) and 250mL of (b):
a) Mix and filter 40mL Tween 80 and 2l0mL 40% isopropanol.
b) Dissolve 5g Na4 EDTA in l50mL H2O add l00mL isopropanol, mix and filter.
Mixed reagent is stable several weeks. Store in non-metal containers.

3. Mineral Oil - paraffin oil, white, light 125/135, saybolt viscosity (38°), specific gravity 0.84-0.86
(24°). Fisher Scientific Co. No. 0-119 or equivalent.

C. Preparation of Sample

1. The number of samples drawn should be six.

2. The sample size shall be 4 - 6 ounces (113 to 170 grams).

D. Procedure

I. Weigh 25.0g of paprika and place in a filter paper cup formed by fitting a 32cm filter paper around
a 400mL beaker. Place cup with ground paprika in a 1L beaker.

2. Pour 400mL 99% isopropanol into the paper cup in the beaker. Place on a pre-heated hot plate,
bring to a boil, then boil gently exactly 10 minutes (a "cold finger" should be used to condense
vapors).

3. Remove cup from beaker without delay and place in a Büchner funnel and aspirate to slow drip.
Discard liquid.

4. Replace cup in 1 liter beaker and repeat Step 2 and 3 twice using 400mL 99% isopropanol each
time to remove oil and pigment.

5. Using a gentle stream of water, quantitatively transfer the sample to a prewashed No. 230 sieve.
Avoid splashing and loss of sample.

18
ASTA ANALYTICAL METHODS

Method 22.1

Microanalytical Analysis of Paprika

6. Wash the sample with a forceful stream of warm (55 -70°C) water using a Fisher aerator until
foam is gone and drainings are clear. Higher flow rates may cause breakage of fragments.

7. Add 400mL 40% isopropanol to wash bottle. Place 6" diameter funnel in trap flask. Wash sample
to the edge of the sieve and quantitatively transfer to the trap flask with 40% isopropanol. Wash
walls of flask and pour remainder of 400mL into flask.

8. Place on hot plate, bring to a boil, then boil gently 10 minutes, using gentle magnetic stirring to
avoid splashing. Wash sides of flask every 2 minutes to prevent material from accumulating and
drying on flask wall.

9. Remove from hot plate and immediately add 100mL premixed Tween 80-40% isopropanol - Na4
EDTA solution down stirring rod.

10. Stir mag., gently, about 1 minute. Let stand 10 minutes.

11. Dilute to 800mL with 40% isopropanol added slowly down stirring rod, positioned with stopper
just above liquid level.

12. Add 50mL mineral oil down stirring rod and stir mag. 3 minutes with stopper located above liquid
level.

13. Add 40% isopropanol slowly down stirring rod to bring oil into neck of flask. Let stand about 10
minutes.

14. Raise stopper to middle of flask and swirl gently to hasten rising of oil droplets.

15. Rinse rod with 40% isopropanol and clamp so that stopper is at mid point of flask.

16. Add 40% isopropanol down rod to bring bottom of oil layer to level 1 cm above raised stopper.

17. Let stand 10 minutes and swirl very gently again.

18. Let stand 10 minutes undisturbed and trap off into beaker, or onto ruled filter paper in Hirsch
funnel.

19
ASTA ANALYTICAL METHODS

Method 22.1
Microanalytical Analysis of Paprika

19. Add 35mL mineral oil and hand stir 1 minute at speed to sufficiently keep oil moving through trap
flask. Add about 20mL 40% isopropanol, stir gently at about 5 minute intervals for 20 - 25
minutes, then let stand undisturbed 5 - 10 minutes.

20. Trap off into second beaker or onto ruled filter paper in Hirsch funnel and rinse neck of flask with
alcohol or undiluted isopropanol.

21. Filter onto ruled paper, rinsing beaker with isopropanol, and examine at 30X.

E. Calculation:

Report separately numbers of insect, rodent hair, animal hair and feather barbule fragments.

F. Statistics:

Repeatability Reproducibility
Rodent hairs 6.41% 8.59%
Elytra squares 5.89% 6.24%

G. Notes

1. Periodically check the 32cm filter paper used under microscope at 30X for completeness of
transfer of fragments

2. When 230 sieve draining slows, wash with detergent, then 50% sodium hydroxide (heated, if
necessary).

3. Complete analysis without overnight interruption.

H. References

AOAC Official Methods of Analysis - 16.14.22 (977.25).


JAOAC 60 114 (1977).

Revised January, 1997

20
ASTA ANALYTICAL METHODS

Method 22.2
Microanalytical Analysis of Ground Capsicums (Excluding Paprika)

Purpose: To isolate extraneous material of insect, rodent, other animal and bird origin
from ground capsicums, excluding paprika, for microscopic detection and enumeration.

A. Apparatus:

1. Stereoscopic binocular microscope - wide field with following minimum specifications: 3 parfocal
objectives - 1X, 3X and 6X or 7.5X; paired 10X wide field oculars, mounted on a base and capable
of illumination by reflected light. Ordinarily 30X magnification is used for routine examination of
filter papers. Confirmation of suspect material at higher magnification may be required.

2. Microscope illuminator - preferably with a transformer or rheostat to vary light intensity, a focusing
adjustment to give uniformly lighted field of view, and blue-white color from a cool low-voltage
source.

3 . Wildman trap flask - consists of a 2L Erlenmeyer flask into which is inserted a close-fitting rubber
stopper supported on a stiff metal rod, 3/16" diam., and about 4" longer than height of flask. Rod is
threaded at lower end and furnished with nuts and washers to hold it in place on the stopper.
Countersink lower nut and washer in the rubber stopper to prevent striking flask.

4. Filter paper: a) 32cm folded rapid flow (S & S 588, or equivalent).


b) 9 cm high wet strength, ruled, 5mm apart (S&S #8 or equivalent).

5. Hirsch funnel - porcelain, 56 mm plate diameter.

6. Büchner funnel, porcelain, 114 mm diameter.

7. Suction flask to provide suction by means of an H2O aspirator or electric vacuum pump.

8. Sieve U.S. Standard No. 230, 8" or 12" diameter (plain-not twill weave).

9. Magnetic stirrer - hot plate.

10. Teflon covered stirring bars about 47mm x 9mm (egg-shaped, round or octagonal)

11. Beakers, glass - 1 liter, funnels, glass or metal, 6" diameter or greater.

21
ASTA ANALYTICAL METHODS

Method 22.2
Microanalytical Analysis of Ground Capsicums (Excluding Paprika)

B. Reagents:

1. Isopropanol (IPA) - 99% and 40% by volume.

2. Ethanol 95% and 60% by volume.

3. Tween 80-ethanol-tetrasodium EDTA Premix: pour 420mL 60% ethanol in 1L graduate. Add
80mL Tween 80 to 250mL glass stoppered graduate. Invert 250mL graduate over 3L beaker and
drain briefly. Rinse 250mL graduate with several portions of the 420mL 60% ethanol, pouring
each into beaker. Add rest of 60% ethanol to beaker and start mag. stirring. Add 10g Tetrasodium
EDTA to beaker while stirring rapidly. Add 500mL 60% ethanol and stir until uniform. Store in
non-metal containers. Mixed reagent is stable several weeks.

4. Mineral Oil - Paraffin oil, white, light 125/135, saybolt viscosity (38°), specific gravity 0.84-0.86
(24°). Fisher Scientific Co. No. 0-119 (or equivalent).

5. Heptane - commercial heptane containing less than 8% toluene.

6. Flotation liquid - mineral oil and heptane (85+15).

C. Preparation of Sample

1. The number of samples drawn should be six.

2. The sample size shall be 4 - 6 ounces (113 to 170 grams).

D. Procedure:

1. Weigh 25 g of capsicum and place in a filter paper cup formed by fitting a 32cm filter paper around
a 400mL beaker. Place cup with ground capsicums in a 1L beaker.

2. Pour 400mL 99% isopropanol into the paper cup in the beaker. Place on a pre-heated hot plate,
bring to a boil, then boil gently 10 min.

3 . Remove cup from beaker without delay and place in a Büchner funnel and aspirate to slow drip.
Discard liquid.

4 . Replace cup in 1 liter beaker and repeat Step 2 and 3 twice using 400mL 99% isopropanol each time
to remove oil and pigment.

22
ASTA ANALYTICAL METHODS

Method 22.2
Microanalytical Analysis of Ground Capsicums (Excluding Paprika)

5. Using a gentle stream of water, quantitatively transfer the sample to a prewashed No. 230 sieve.
Avoid splashing and loss of sample.

6. Wash the sample with a forceful stream of warm (55-70°C) water using a Fisher aerator until foam
is gone and drainings are clear. Higher flow rates may cause breakage of fragments. (Note: Longer
washing time than for paprika is needed.)

7. Add 600mL 60% ethanol to wash bottle. Place 6" diameter funnel in trap flask. Wash sample to
the edge of the sieve and quantitatively transfer to the trap flask with 60% ethanol. Wash walls of
flask and pour remainder of 600mL into flask.

8. Place on hot plate, bring to a boil, then boil gently 10 minutes, using gentle magnetic stirring to
avoid splashing. Wash sides of flask every 2 minutes to prevent material from accumulating and
drying on flask wall.

9. Remove from hot plate and cool to between 20 and 25° with cold water. Add 40mL flotation
liquid down stirring rod.

10. Dilute to 800mL with 60% ethanol and stir mag. 5 minutes.

11. Set aside, add 100 mL Tween 80-ethanol-tetrasodium EDTA premix, down stirring rod, and mix
through liquid by gently swirling (to prevent foaming) stopper about 1 minute. Let stand 3
minutes. Wash sides of flask with 60% ethanol to keep solids down.

12. Slowly add 60% ethanol down trap rod, maintaining stopper above oil layer, until oil just reaches
neck of flask.

13. Gently swirl stopper through lower portion of flask to suspend settling.

14. Add 60% ethanol down rod to bring bottom of oil layer to a level 1 cm above raised stopper.

15. Clamp rod with stopper at mid point of flask. Let stand 15 minutes. Then gently swirl stopper
through upper half of liquid to hasten rising of oil droplets.

16. Let stand 15 minutes undisturbed and trap into beaker, rinsing neck of flask with 60% ethanol.
Filter onto ruled paper.

17. Add 30mL flotation liquid and stir manually 1 minute, with an up and down motion.

23
ASTA ANALYTICAL METHODS

Method 22.2
Microanalytical Analysis of Ground Capsicums (Excluding Paprika)

18. Clamp rod at mid point and let stand 10 minutes. Swirl stopper gently through upper half of liquid
and adjust oil level.

19. Let stand 15 minutes undisturbed and trap off.

20. Rinse neck of flask with 95% ethanol.

21. Filter onto ruled paper, rinsing beaker with 95% ethanol, and examine at 30X.

E. Calculation:

Report numbers of insect, rodent hair, animal hair and feather barbule fragments.

F. Statistics:

Repeatability Reproducibility
Rodent hairs 13.43% 14.66%
Elytra squares 8.10% 9.18%

G. Notes:

1. Periodically check the 32cm filter paper used under microscope for completeness of transfer of
fragments.

2. When 230 sieve draining slows, wash with detergent, then 50% sodium hydroxide (heated if
necessary).

3. Complete analysis without overnight interruption.

4 Do not use any plastic equipment because fragments or hairs might adhere.

H. Reference:

AOAC Official Methods of Analysis 16.14.10 (978.22).


JAOAC 61 900 (1978).

Revised January, 1997

24
ASTA ANALYTICAL METHODS

Method 26.0
Sumac in Oregano

Purpose: To determine the presence of sumac in oregano.

A. Apparatus:

1. Stereoscopic binocular microscope--widefield with the following minimum


specifications: 3 parfocal objectives--1X, 3X and 6X or 7.5X; paired 10X widefield oculars,
mounted on a base and capable of illumination by transmitted or reflected light. Ordinarily 30X
magnification is used for routine examination of filter papers. Confirmation of suspect material at
higher magnification may be required.

2. Compound polarizing microscope - microscope with the following minimum


specifications: 4 parfocal achromatic objectives of ca 4, 10, 20, and 40X; revolving 4-place
nosepiece; Abbe condenser with N.A. of 1.25; 10X Huygenian or widefield eyepieces; fine
adjustment; mechanical stage; fitted with polarizing prisms below and above the mechanical stage.

3. 100 mm Petri plates.

4 . 7 cm (or 9 cm) ruled filter papers.

5. Microscope slides and cover slips.

6. Eye dropper.

7. Dissecting needle and forceps.

B. Reagents:

1. Xylene - reagent grade.

C. Preparation of Sample:

1. Utilize sample procedures for original sampling (see Method 14. 1). From each sub-sample, take a
representative 10 g (approximately 75 mL) sample of oregano leaf. These samples will be
composited and gently blended.

2. Prepare a 5 to 10 g analytical sample from above using a sampling splitter or quartering procedure.

3. Maintain leaf integrity; do not break up leaves.

25
ASTA ANALYTICAL METHODS

Method 26.0
Sumac in Oregano

D. Procedure:

1. Gently shake enough oregano into one Petri plate lined with standard 7 cm (or 9 cm) ruled filter
paper to cover the filter paper in a single layer (approximately 500 leaf fragments per plate; in no
case is less than 400 mg of oregano fragments to be viewed).

2. Examine the plate of material under the 30X to 60X magnification of the stereoscopic binocular
microscope looking for the following distinguishing characteristics:

Oregano - Oil glands, jointed hairs


Sumac - No oil glands, single cell hairs with central cavity

3. If no sumac is found in the plate, report as "Sumac Negative."

4. If sumac is found in the plate, report as Presumptive Sumac Positive (PSP) and continue to the
confirmatory steps.

5. To confirm the presence of sumac, place leaf fragments of oregano and the PSP material on a
microscope slide and place a cover slip over the material. Using an eye dropper, introduce enough
xylene to fill the cover slip.

6. Polarizing Microscope -
Observe with crossed polars at 40X to 100X magnification for the following:

Oregano - No oxalate crystals


Sumac - Oxalate crystals, birefringence of the sumac hairs and their central
cavity. (Note)

7. If the presence of sumac is confirmed, report as "sumac positive".

E. Calculation:

N/A

F. Statistics:

N/A

G. Notes:

Upon removing the polarization, the oxalate crystals in the sumac disappear.

H. References:

N/A Revised January 1997

26
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